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ĐẠI HỌC BÁCH KHOA HÀ NỘI LUẬN VĂN THẠC SĨ Nghiên cứu tái sử dụng phế thải nông nghiệp làm vật liệu hiệu cao xử lý nước thải PHẠM VĂN HỒNG Hoang.PV202815M@sis.hust.edu.vn Ngành Kỹ thuật mơi trường Giảng viên hướng dẫn: PGS TS Thái Yên Ch ký ca GVHD Viện: Khoa hc Công ngh ng HÀ NỘI, 4/2023 CỘNG HÒA XÃ HỘI CHỦ NGHĨA VIỆT NAM Độc lập – Tự – Hạnh phúc BẢN XÁC NHẬN CHỈNH SỬA LUẬN VĂN THẠC SĨ Họ tên tác giả luận văn: Ph Đề tài luận văn: Nghiên cu tái s dng ph thi nông nghip làm vt liu hi c thi Chuyên ngành: K thung Mã số SV: 20202815M Tác ging dn khoa hc H ng chm lu xác nhn tác gi a cha, b sung lun hp Hng ngày 28/04/2023 vi ni dung sau: - - Vit li phn kt lung bao quát ni dung nghiên cu kèm kt qu ng; B sung thêm phn 1.4.3 Quá trình hp ph bt u t trang 27 vi ni dung: i hp ph; ca trình hp ph; Các yu t n trình hp ph B sung danh mc t vit tt vi PVA WCA; Thay th th dng thành dng ct vi hình 30 31; Vit hóa thut ng ti trang 9; B sung trích dn tài liu tham kho vi hình t n 10; B sung mơ t v lp thí nghim Ngày 23 tháng 2023 Giáo viên hướng dẫn Tác giả luận văn CHỦ TỊCH HỘI ĐỒNG ĐỀ TÀI LUẬN VĂN Nghiên cu tái s dng ph thi nông nghip làm vt liu hi c thi ng dn Ký ghi rõ h tên Lời cảm ơn Em xin bày t lòng bi Thái Yên ng dn to mu kin tt nh em thi gian thc hin Lu Em xin gi li co vin, phòng ban, thy cô ca b môn Công ngh ng, B môn Qung phịng thí nghim Vin Khoa hc Cơng ngh n dy kin thc to mu kin v vt ch th t em hoàn thành ni dung nghiên cu ca Lu Cuc bày t lòng bin nh nhng thy cơ, bng tình cng viên, chia s sut trình hc tp nghiên cu HC VIÊN Ký ghi rõ h tên Tóm tắt luận văn Nguc h a nghiêm trng bi ô nhim du t s c tràn du trình thi b du thy vc, t vic ch to loi vt liu hi i loi b hiu qu ng dc c nhiu s quan tâm Vt liu cellulose aerogel t thc vt cho thy nhiu ti có kh y sinh hc, hp ph du kh o ca cellulose Trong nghiên cu này, cc tng hp t loi ph thi nơng nghi, bã mía d s dng cho mu khc nhim du Quy trình tng hp cellulose aerogel gn vi mc tiêu s dng dung mơi c hi Thay tn theo quy trình chit Soxhlet s dc hc chit tách t loi vt liu thơ bm hóa s dng NaOH vi s h tr ca sóng siêu âm Cellulose c s d ng làm tin ch ch t to tính k c cho ng dng hp ph du hn hp du c, mu cellulose aerogel t c ph vi methyltrimethoxysilane (MTMS)m: SEM, c (WCA) c s d c tính ca vt liu cellulose aerogel Mu cellulose aerogel c kim tra kh p ph du thông qua vinh dung ng hp ph vi du nht thi du diesel nguyên chtáp dng vi h du c Các yu t n trình hp ph du hn hp du c ca cellulose aerogel bao gm: khng vt liu aerogel, thnhi c ki ng hc gi bc 1, bc mơ hình Elovich c áp d mơ t ng hc ca q trình hp ph dc Kt qu cho thy rng mu cellulose aerogel to thành có kh dng rõ ràng mà khơng b v cu trúc mng cu trúc ba chi n hình c rt nh, khng t 15.4252.63 mg/cm3 rng xp cao (95.8298.97%) ng hp ph du nguyên cht 27.81 g/g vi du nht thi 26.85 g/g vi du diesel t 110o th hin tính k c ca cellulose aerogel sau trình ph MTMS Các mu cellulose aerogel d dàng ni b mc hp ph du vng hp ph du nht tht 27.49 g/g, giá tr vi du diesel 25.29 g/g V ng ca khng vt liu, dung ng hp ph vi c loi dng gim khng vt liu 0.05 g lên 0.45 g Mơ hình gi ng hc bc mơ hình Elovich mơ t ng hc ca q trình hp ph du nht thi du diesel tt vi h s i nhi, ng ging hp ph c quan sát thy nhi khong 1060 o C, kt qu c ng ca nhi nht ca du Quá trình hp ph du nht thi du diesel ca cellulose aerogel không b nh ng bi giá tr pH ca hn hp du c thơng qua thí nghim vi giá tr pH thay i t 3, 5, bn kh dng cc khnh vi 10 ln hp ph nh hp ph liên tc MỤC LỤC DANH MỤC HÌNH .1 DANH MỤC BẢNG BIỂU DANH MỤC TỪ VIẾT TẮT ĐẶT VẤN ĐỀ .4 CHƯƠNG TỔNG QUAN 1.1 Tổng quan aerogel 1.1.1 Khái niệm đặc tính 1.1.2 Phân loại .8 1.2 Aerogel sinh học .9 1.3 Cellulose aerogel từ sinh khối thực vật 12 1.3.1 Cellulose nguồn cellulose từ sinh khối thực vật 12 1.3.2 Quy trình chế tạo cellulose aerogel 14 1.3.3 Ứng dụng cellulose aerogel 18 1.4 Cellulose aerogel ứng dụng xử lý nước nhiễm dầu 21 1.4.1 Nước thải nhiễm dầu 21 1.4.2 Nước nhiễm dầu cố tràn dầu 24 1.4.3 Quá trình hấp phụ .26 1.4.4 Các công bố ứng dụng vật liệu cellulose aerogel xử lý nước nhiễm dầu 30 CHƯƠNG VẬT LIỆU VÀ PHƯƠNG PHÁP NGHIÊN CỨU 34 2.1 Vật liệu .34 2.1.1 Các loại sinh khối sử dụng để chiết tách cellulose .34 2.1.2 Đối tượng ứng dụng xử lý 34 2.2 Quy trình chế tạo cellulose aerogel từ sinh khối thô 34 2.2.1 Chiết tách sinh khối thu cellulose 34 2.2.2 Gel hóa hỗn hợp cellulose – PVA 35 2.2.3 Đông khô tạo aerogel 35 2.2.4 Tạo lớp phủ kị nước cho aerogel 36 2.3 Xác định đặc tính vật liệu 36 2.3.1 Đặc điểm hình thái cấu trúc 36 2.3.2 Khối lượng riêng độ xốp 37 2.3.3 Diện tích bề mặt riêng 37 2.3.4 Tính thấm nước .38 2.4 Thí nghiệm hấp phụ nước dầu 38 2.5 Thí nghiệm hấp phụ dầu hỗn hợp dầu – nước 39 2.5.1 Ảnh hưởng khối lượng cellulose aerogel đến hiệu loại bỏ dầu 39 2.5.2 Ảnh hưởng thời gian tiếp xúc động học hấp phụ 39 2.5.3 Ảnh hưởng nhiệt độ 40 2.5.4 Ảnh hưởng pH 40 2.6 Thí nghiệm đánh giá khả tái sử dụng 41 CHƯƠNG KẾT QUẢ VÀ THẢO LUẬN 42 3.1 Xác định đặc tính vật liệu 42 3.1.1 Đặc điểm hình thái bề mặt 42 3.1.2 Cấu trúc tinh thể nhóm chức 43 3.1.3 Khối lượng riêng độ xốp 45 3.1.4 Diện tích bề mặt riêng kích thước mao quản 46 3.1.5 Tính kị nước 47 3.2 Dung lượng hấp phụ với nước dầu nguyên chất .49 3.3 Dung lượng hấp phụ dầu hỗn hợp dầu – nước 53 3.3.1 Ảnh hưởng khối lượng cellulose aerogel .53 3.3.2 Ảnh hưởng thời gian tiếp xúc động học hấp phụ 54 3.3.3 Ảnh hưởng nhiệt độ 56 3.3.4 Ảnh hưởng pH 57 3.3 Khả tái sử dụng aerogel 58 3.4 So sánh với loại vật liệu hấp phụ tổng hợp khác .59 KẾT LUẬN 61 TÀI LIỆU THAM KHẢO 62 PHỤ LỤC 70 DANH MỤC HÌNH Hnh Lch s hình thành phát trin ca vt liu aerogel [6] Hc tính ca aerogel [7] Hnh Phân loi aerogel [3] Hnh Quy trình ch to aerogel sinh hc [7] .10 Hnh Cellulose t sinh khi thc vt [10] 13 Hnh Mi quan h gic mao qun nhi [10] .16 Hn chuyn khi trình hp ph [45] 28 Hnh Cellulose aerogel tng th phân loi aerogel [10] 31 Hnh Quá trình tách tái sinh du/dung môi hi b du/dung môi hu ng u (b) Lc hn hp du c bng c (c) Tái to aerogel bt ép [10] 32 Hnh 10 (A) Quy trình chung ch to aerogel da cellulose, (B) Loi b du mc bng aerogel thu hi du bi, tr lu ca cellulose aerogel sau nén [54] 32 Hnh 11 Ph thi nông nghin cung c, b) Bã mía c) Lá da 34 Hnh 12 (a) Quá trình tin x lý bng sóng siêu âm (b) Hn hp sau q trình kim hóa 35 Hnh 13 Quy trình ch to cellulose aerogel t sinh khi 35 Hnh 14 (a) Khuôn cha gel (b) Các mkhô 36 Hnh 15 nh SEM ca mu aerogel cha 0.5 wt% cellulose: a) A- MTMS, b) A- MTMS, c) A- MTMS, d) A- MTMS, e) nh SEM ca bt da thô f) Các mu aerogel thành phm .42 Hnh 16 Ph FTIR ca loi sinh khi thô, m ph MTMS, A-RR ph MTMS du nht thi 44 Hnh 17 Ph nhiu x tia X (XRD) ca mu sinh kh MTMS A-RR ph MTMS 45 Hnh 18 (a) Kh xp ca mu cellulose aerogel sau ph MTMS vi s i ca n cellulose (bi dng ct bi dng ng lt ng vi giá tr Kh rng xp) (b) Mu cellulose aerogel nm nhy ca hoa Ly 46 Hng nhit hp ph nh hp ph N2 vi mu A MTMS b) ph MTMS 47 Hnh 20 a) Ging b mt cellulose aerogel ph MTMS du nht du diesel d dng b hp ph, b) c) Cellulose aerogel ph MTMS d dàng ni lên b mc sau b nhúng chìm .48 Hnh 21 Giá tr WCA a) ti b mt ngoài, b) ti mt ct bên cellulose aerogel ph MTMS 48 Hnh 22 Quá trình hp ph du nguyên cht theo thu tiên 49 H ng hp ph d ng cellulose ca mu cellulose aerogel ph MTMS 50 Hng hp ph ca cellulose aerogel 0.5 wt% ph MTMS vi du nht du diesel nguyên cht theo thi gian .51 Hng hc hp ph ca mu A-RR 0.5 wt% ph MTMS vi du nht du diesel nguyên cht 51 H ng hp ph du vi m c sau ph MTMS 52 Hnh 27 Quá trình cellulose aerogel ph MTMS hp ph du nht thi hn hp du c .53 Hnh 28 ng ca khng hp ph du nht thi du diesel 54 Hng hc hp ph ca mu A-RR 0.5% ph MTMS vi du nht thi du diesel hn hp du c 54 Hnh 30 ng ca nhi n hiu sut hp ph du nht thi du diesel ca cellulose aerogel 57 Hnh 31 ng cng hp ph du nht thi du diesel .58 Hng hp ph hiu sut tách du sau 10 chu k hp ph - nh hp ph bc 59 Hnh 33 Cellulose aerogel ph MTMS ti thi c sau 10 ln tái s dng liên tip 59 DANH MỤC BẢNG BIỂU Bng Thành ph, bã mía da 14 Bt tách cellulose ch tng 17 Bng Các công ngh x lý dc [1] 23 B lý s c du tràn [43] 25 Bng So sánh hp ph vt lý hp ph 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(%) 0.57 98.81 0.48 97.87 0.54 95.82 Ghi chú: SD (Standard Deviation) lch chun Bảng ng hp ph du nguyên cht ng cellulose ca aerogel ph MTMS Mẫu wt% A-RR 0.5 27.81 23.63 22.7 0.5 26.85 20.97 18.83 SD A-BM Dầu nhớt thải (g/g) 0.38 26.16 0.63 23.92 0.42 20.88 Dầu diesel (g/g) 0.35 26.5 0.57 18.67 0.45 19.41 SD A-LD SD 0.37 0.45 0.69 27.08 21.75 22.84 0.38 0.68 0.34 0.39 0.46 0.48 25.85 19.74 18.43 0.49 0.62 0.56 Bảng ng hp ph du nguyên cht vi mu cellulose aerogel 0.5% c sau ph MTMS Mẫu A-RR 24.34 27.81 23.42 26.85 SD A-BM Dầu nhớt thải (g/g) 0.46 23.99 0.38 26.16 Dầu diesel (g/g) 0.75 21.77 0.35 26.5 70 SD A-LD SD 0.65 0.37 23.34 27.08 0.67 0.38 0.87 0.39 22.69 25.85 0.35 0.49 Bảng ng ca khng hp ph du hn hp du c Khối lượng cellulose aerogel (g) Dung lượng hấp phụ (g/g) Dầu nhớt thải 27.94 26.87 22.69 19.71 19.04 18.45 18.77 18.21 Dầu Diesel 25.58 23.25 22.28 19.35 19.81 18.30 18.09 18.12 0.0501 0.0848 0.1233 0.1736 0.2568 0.3484 0.3864 0.4289 0.0557 0.0908 0.1183 0.1702 0.2636 0.3532 0.3907 0.4212 Hiệu suất (%) 17.50 28.48 34.96 42.77 61.11 80.33 90.65 97.61 17.81 26.39 32.95 41.17 65.28 80.80 88.33 95.42 Bảng ng hp ph du c ca cellulose aerogel ph MTMS theo thi gian Dầu nhớt thải Dầu Diesel Thời gian (phút) Dung lượng hấp phụ (g/g) Thời gian (phút) Dung lượng hấp phụ (g/g) 0.16667 0.5 10 20 30 35 0.00 5.33 12.71 18.25 22.77 26.26 27.81 27.55 27.49 27.56 0.08333 0.16667 0.33333 10 20 30 0.00 23.71 24.30 24.58 24.83 25.02 25.09 25.24 25.25 25.29 71 Bảng ng ca nhi n hiu sut hp ph du hn hp du c ca cellulose aerogel ph MTMS Dầu nhớt thải Nhiệt độ (o C) Dầu Diesel Dung lượng hấp phụ (g/g) SD Dung lượng hấp phụ (g/g) SD 26.13 27.56 27.12 25.34 24.39 0.79 1.15 0.64 0.31 0.22 26.79 25.65 25.09 24.38 22.88 1.12 0.83 0.67 0.56 0.65 10 20 25 40 60 Bảng ng cng hp ph du hn hp du c ca cellulose aerogel sau ph MTMS pH 27.38 26.21 27.12 26.48 27.45 26.84 27.65 26.46 Loại dầu Diesel Bảng ng hp ph hiu sut tách du sau 10 chu k hp ph nh hp ph bc Số lần tái sử dụng Dung lượng hấp phụ (g/g) 10 27.38 11.78 7.27 6.51 6.56 5.96 6.30 6.26 6.28 6.22 6.20 25.42 15.43 7.83 SD Dầu nhớt thải 0.36 0.19 0.04 1.06 0.62 0.84 1.04 0.99 1.00 1.02 1.00 Dầu Diesel 0.33 0.22 0.37 72 Hiệu suất tách dầu (%) SD 65.01 45.92 35.66 33.75 35.27 32.90 34.90 35.01 35.07 34.72 34.63 5.36 5.36 4.75 0.10 2.15 0.30 0.67 0.77 0.77 0.89 0.89 72.23 59.18 44.65 2.13 1.38 0.92 10 7.36 7.34 7.07 6.65 6.56 6.53 6.49 6.43 0.68 0.47 0.63 0.43 0.43 0.44 0.42 0.36 73 42.95 43.59 43.06 41.35 41.49 41.50 41.51 41.38 2.21 1.60 1.92 1.03 1.37 1.58 1.47 1.21 TÓM TẮT LUẬN VĂN THẠC SĨ tài: Nghiên cu tái s dng ph thi nông nghip làm vt liu hi c thi Tác gi lu Khóa: 2020B ng d Thái Yên T khóa (Keyword): , bã mía, da, vt liu cellulose aerogel, hp ph du Ni dung tóm tt: a) Lý ch tài Vt liu cellulose aerogel t thc vt cho thy nhiu ti hy sinh hc, hp ph du kh o ca cellulose Hp ph c coi mt công ngh hiu qu x c thi nhim du kh i b du cao, d vn hành tiêu th ng Các vt liu hp ph truyn thng bao gm polypropylene (PP), zeolit than hot tính, nhiên nhng vt liu có nh kh dng kém, kh p ph d chn lc thiu kh phân hy sinh hc Vic nông nghip vi din tích canh tác dành lúa c, mía da chim mt t trng lu nn nông nghi mng ln ph thi nông nghi i v mùa thu hoch ng sinh khi mang tin, yêu cu bc thit s dng có hiu qu ng ph thy, có th thu hng sinh khi làm ngun nguyên li sn xut cellulose aerogel ng dng x c nhim du b) Mu ca lung, phm vi nghiên cu Mục đích nghiên cứu Ch to thành công vt liu aerogel nn cellulose t loi ph thi nơng nghip g, da bã mía có kh p ph du hiu qu Đối tượng phạm vi nghiên cứu - Ph thi nông nghi, bã mía da Vt liu hi c thc nhim du (du nht thi du diesel) Nội dung nghiên cứu - Ch to cellulose aerogel vi n i t 0.5 wt%, wt% wt% vc chit tách t loi ph thi nơng nghi, bã mía da; c tính ca mu cellulose aerogel ch tc, bao gm: cu trúc hình thái, cu trúc tinh th nhóm ch xp, tính k c; - ng hp ph hai loi du (du nht thi du diesel) ca cellulose aerogel; - ng dng cellulose aerogel trình hp ph du hn hp du c: Nghiên cu ng ca yu t: khng cellulose aerogel, thi gian phn ng, nhi ng hp ph du nht thi du diesel; Nghiên cu kh dng hiu qu tách du ca cellulose aerogel sau q trình hp ph c) Tóm tng ni dung i ca tác gi - Vt liu cc tng hp t loi ph thi nông nghi, bã mía d x c thi nhim du có nhic tính ni tri v kh p ph Hiu qu ca trình cht tách cellulose t sinh khi c nâng cao nh áp dng quy trình tin x lý bng sóng siêu âm Sau q trình chit tách này, hemicellulose c loi b hoàn toàn Các mu cellulose aerogel to thành có kh ng rõ ràng mà không b v cu trúc mng cu trúc ba chin hình, bênh cng riêng th rng xp cao Vt liu aerogel có tính k c nh q trình sylan hóa b mt s dng methyltrimethoxysilane (MTMS) dàng ni mt c hp ph du Sau kim tra ng ca yu t: khng vt liu, thi gian hp ph, nhi c kim tra kh dng bng ép c d) u Thay áp dng quy trình chit Soxhlet s dc hi (toluen), cellulose c chit tách t loi vt liu thơ bm hóa s dng NaOH vi s h tr cc s dng làm tin ch ch t- to tính k c cho ng dng hp ph du hn hp du c, mu cellulose aerogel to thành c ph v c s d c tính ca cellulose aerogel sau ph MTMS Mc king hp ph vi du nht thi du Diesel nguyên chc ng dng vi h du c Các yu t n trình hp ph du hn hp du c bao gm: khng cellulose aerogel, th c ki ng hc gi bc 1, bc áp d mơ t ng hc ca q trình hp ph du c e) Kt lun c ch to thành công t loi ph thi nông nghip gm , bã mía da c loi b hồn tồn sau trình chit tách thu cellulose nh trình kim hóa tin x lý bng sóng siêu âm c rt nh (15.4252.63 mg/cm3) có rng xp cao (95.82 98.97%) ng hp ph du nguyên cht 27.81 g/g vi du nht thi 26.85 g/g vi du diesel Sau q trình ph MTMS, vt liu có tính k c d dàng ni b mng thi hp ph du nht thi du diesel vng hp ph du nht tht 27.49 g/g, giá tr vi du diesel 25.29 g/g V ng ca khi ng vt ling hp ph vi c loi dng gim khi ng vt li 0.05 g lên 0.45 g Mô hình gi ng hc bc mơ hình Elovich mơ t ng hc ca q trình hp ph du nht thi du diesel tt vi h s quan cao Vi nhing ging hp ph c quan sát thy nhi ng 1060 oC, kt qu c ng ca nhi lên nht ca du Quá trình hp ph du nht thi du diesel ca cellulose aerogel không b ng bi giá tr pH ca hn hp du c thơng qua thí nghim vi giá tr i t 3, 5, Cellulose aerogel có th c s dng li nhiu vịng (~10 ln) thu hi du nh n Kt qu c cho thy rng cellulose aerogel t loi ph thi nơng nghip có nhc tính hp ph du hiu qu, cho thy ting dng vic tách du khi nhiu nguc ô nhim, k c s c tràn du hoc x c nhim du
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